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Sodium Hydroxide → HCID 69357330、化合物

HRID 852544
ノート
印刷プレビュー

反応式

HRID 852544 の反応式
[CH3:1][O:2][C:3](=[O:17])[C:4]1[CH:13]=[C:12]([O:14][CH2:15][CH3:16])[CH:11]=[C:6]([C:7]([O:9]C)=[O:8])[CH:5]=1.[OH-].[Na+]>CO>[CH3:1][O:2][C:3](=[O:17])[C:4]1[CH:13]=[C:12]([O:14][CH2:15][CH3:16])[CH:11]=[C:6]([C:7]([OH:9])=[O:8])[CH:5]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 68538880HCID 68538880、化合物

生成物 1

HCID 69357330HCID 69357330、化合物収率 82.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of 5-ethoxy-isophthalic acid dimethyl ester (D43) (22 g, 92.4 mmol, 1 equiv) in MeOH (440 ml) was added 1N aqueous NaOH solution (87.8 ml, 87.8 mmol, 0.95 equiv) and the resulting solution was stirred at room temperature for 17 h. Most of the MeOH was removed in vacuo and the residue was partitioned between AcOEt and 1N aqueous NaOH solution. The aqueous layer was extracted with AcOEt, acidified to pH 1 and re-extracted with AcOEt. The second organic extract was dried over MgSO4 and concentrated in vacuo to give 5-ethoxy-isophthalic acid monomethyl ester (D45) (17 g, 82%) as a white solid. [M+H+ NH3]+=242.0, RT=2.79 min

後処理

  1. customMost of the MeOH was removed in vacuo
  2. customthe residue was partitioned between AcOEt and 1N aqueous NaOH solution
  3. extractionThe aqueous layer was extracted with AcOEt
  4. extractionre-extracted with AcOEt
  5. extractionThe second organic extract
  6. dry with materialwas dried over MgSO4
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-78fa2a39409a4fab9a8b2293e0d49f36
出典データセット
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07253198B2

反応ノート

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